“A Novel Real Time Quantitative Analytical Spectroscopy Technique for Analyzing All the Congeners Emerging from a Distillation Process” by Robin Felder, PhD
Sole Proprietor Monte Piccolo Farm and Distillery
3135 Blandemar Dr.
Charlottesville, VA 22903
The University of Virginia, Professor of Pathology, Associate Director Laboratory Medicine
Chair, Medical Automation.org
Founder and President, Association for Laboratory Automation (now SLAS)
What area of research are you performing?
The use of fast Fourier molecular rotation spectroscopy (FFMRS) to analyze and improve the heads/heart “cut” in craft distilling volatile distillation congeners in real time during a distillation run. I am collaborating with the Chemistry Department at the University of Virginia (Charlottesville, VA) to test the ability of the novel FFMRS technology to measure the molecular content of the heads and hearts of pear eau-de-vie style fresh pear brandy. Normally, the heads and hearts “cut” is made at sensory discretion of the distiller. The “cut” can vary greatly based on the olfactory acuity of the distiller and the content of the fruit due seasonal variation. Distillers would appreciate an objective measure of their distilling skills, or to improve their distilling skills such as when and how much offensive compounds like acetaldehyde, methanol, butanol are emerging from their process and when and how much pleasant fruit esters such as ethyl 2,4 decadienoate (EDDO) are emerging. I have been researching methods to measure molecules in the distillation vapor before and immediately after it emerges from the still. Traditional methods are either not sufficiently definitive (gas chromatography), too expensive and laborious (mass spectrometry), or haven’t been invented yet.
Fortunately, along comes the invention of the FFMRS instrument and associated software by my colleague Brooks Pate PhD. He was awarded the most notable award at our university, The Innovator of the Year, due to this invention. Is has been recently commercialized and is in use by the pharmaceutical industry to test the purity of raw materials destined to be the drugs approved by the FDA. As a craft distiller/scientist it became obvious to me that FFMRS could probably revolutionize the distillation industry, particularly the distillation of spirits.
Because of the high spectral purity of microwave light sources and high dynamic range, Chirped Pulse Fourier Transform Microwave (CP-FTMW) spectroscopy, also known as FFMRS, provides unparalleled ability to unambiguously determine molecular structure. Since the rotational transition frequencies of a given species are determined purely by the moments of inertia of the molecule, mass shifts due to isotopic substitution generally cause relatively large shifts in transition frequency with respect to the spectral resolution. The acquisition and assignment of isotopically substituted spectra of a target species allow us to determine, with application of Kraitchman’s equations or least linear squares fitting (see OSU ISMS talk: 2012 RH03), accurate experimental molecular structures with precision at the level of a few picometers. Thankfully, the high dynamic range of CP-FTMW generally allows for detection of the most common heavy atom isotopologues in natural abundance, as well. For representative results, see recent talks in the Publications section of my collaborator and colleague Brooks Pate PhD. http://faculty.virginia.edu/bpate-lab/cpftmw.html
Reason and history behind the proposal
Brandy distillation is a particularly challenging art due to the complexity associated with growing ideally ripened fruit, managing an ideal fermentation, followed by a skilled distillation. Normally, the heads and hearts “cut” is made at sensory discretion of the distiller. The “cut” can vary greatly based on the olfactory acuity of the distiller and the content of the fruit due seasonal variation. Distillers would appreciate an objective measure of their distilling skills such as which offensive compounds when and how much offensive compounds like acetaldehyde, methanol, butanol are emerging from their process and when and how much pleasant fruit esters such as ethyl 2,4 decadienoate (EDDO) are emerging. Award winning pear brandies in Europe have concentrations of EDDO well over the flavor threshold for expert testers. In other words, if one knows the concentration and identity of award winning esters as the distillation is progressing, one can decide how to adjust the process or back blend the products in order to improve the tasting experience for the consumer.
I learned about this technology when I was attending UVAs Innovator of the Year Award ceremony a few years ago, invited as UVA’s first recipient. We launched a collaboration the following year and performed analyses on my distillations. The results were unequivocal which demonstrated the value of this technology to distillers. Since the price of these instruments are dropping precipitously due to improvements and reduced cost of electronics it seemed appropriate to launch a more intensive investigation into the versatility of the FFMRS. Your grant opportunity has eclipsed my interest in moving forward.
Why is this important and what goes before it? Is there anything already published on it?
This technology has been published, commercialized, and has received awards (UVA’s Innovator of the Year, 2016). http://faculty.virginia.edu/bpate-lab/cpftmw.html However, it is relatively little known since it takes time for novel instrumentation to penetrate existing markets despite the vast improvements it brings to parameters such as sensitivity, selectivity, speed, and ultimately cost. Our preliminary work in my distillery has demonstrate unequivocally that it brings hard data to the art of distilling. We plan on generating two distillation focused publications in peer reviewed literature to serve as a foundation for our future work in this area. The first publication is almost completed. In order to popularize FFMRS we need to work with an organization such as the ADI that has a wide following and is a notable voice in distilling.
What prompted you here? References should be included (required)
I was prompted to look into the mission and opportunities at the ADI since I am a new distiller who is about to open his doors. I’ll be joining the ADI as suggested by my instructors and collaborators:
Dave Pickerell PhD, Managing Director Oak View Consulting, Louisville, KY (formerly Makers Mark)
Ian Glomski PhD, Vitae Sprits, Charlottesville, VA
Denver Riggleman, US Virginia Congressman (5th District), Owner Silverback Distillery
Alex Toomy, Owner Ragged Branch Distillery, Charlottesville, VA
Lyons Brown MBA (UVA Darden Business School graduate), Former chairman and chief executive officer of Brown-Forman Corporation, currently Altamar Brands, Charlottesville, VA
What do you hope to achieve this year?
Month 1 – 3 – Collect specimens on site at Vitae, Monte Piccolo, and Silverback distilleries to assure proper sampling, quality control, and labeling.
Month 4- 6 – Analyze the specimens in triplicate, perform data reduction, statistical analysis, and validation with analytical statisticians and scientific distillers (Ian Glomski PhD and Dave Piccerell PhD)
Month 6-12 – We will write and submit for publication our scientific articles. We will also write, as required, the article for the ADI. If the budget allows we will expand the scope of our sample collection to include bourbon and rye whisky, varietal gins ™, and expand the fruit selection of brandies. This grant will allow us to launch this project so that it can write additional grants to fully vet the use of FFMRS in a wide variety of distilling arenas from the smallest craft distilleries to large commercial distilleries through my connection with one of the principle owners of the Browns Forman Corporation. I have been successful in raising over $70M in grants from the National Institutes of Health over the last 40 years.
How will you attempt to do this (internal, external lab)?
The laboratory of Dr. Brooks Pate PhD (inventor of FFMRS) has been in operation for over a decade. He has built two of the first few FFMRS instruments in the World. These research full spectrum spectrometers are designed to identify any and all relatively small compounds in volatile liquids (such as the effluent from a still). Once the compounds from distillations have been catalogued, then smaller less expensive instruments can be used specifically for distillation where side sampling of liquid or vapor streams is possible. For example, fruit esters in brandies are generally under 10 carbons and thus are much easier and faster to quantify (real time) than compounds in pharmaceuticals.
Where will the money be spent?
The money will be used to pay for the disposables associated with collecting and analyzing the effluents of the stills at Monte Piccolo, Vitae Spirits, and Silverback Spirits distilleries. Specimen analysis fees will be paid to the laboratory of Dr. Brooks Pate PhD who maintains several FFMRS instruments at The University of Virginia. (see budget at the end of this proposal)
How will you interpret the results?
Use standard materials (e.g. acetaldehyde, methanol, butanol, propanol, 2,4 decadieneoate, etc.) obtained commercially already on the shelf at Monte Piccolo Distillery to validate the results as we have in our preliminary studies. We will also analyze some notable European Williams pear brandies (e.g. Poire William, Morand Family, Martigny Switzerland, Rochelt Spirits, Innsbrook Austria) since these are the fruit brandies on which scientific literature has been published. FFMRS is unique in being able to positively identify and quantify all but the most very large and complex congeners found in most analytical processes. Blind smelling and tasting with local distillers will be performed and quantified using the flavor wheel approach to determine how far off some individuals will be in classifying their distillates. Professional tasters will be available at the Browns Forman Corporation (personal communication from Lyons Brown to Robin Felder) to see how their impressions differ from our local craft distillers.
If successful with the findings how should research process further or what will this contribute to the distilling field?
We have demonstrated in a 2016 academic year long student project that the FFMR instrument can be instrumental in improving the quality control of craft level distilled spirits. Based on this preliminary data and resulting publications (in preparation), we will be applying for grants from the National Science Foundation and crowd sourcing funds from large commercial distillers. Dr. Felder has generated over $70M in federal funding and published over 300 publications during his research career. He will ultimately retire full time into his craft distillery and use his scientific knowledge to further art and science of craft distilling.
Specimen collection disposables: gloves (prevent human contamination), screw cap tubes, pipettes, marking pens, sequentially labelled bar codes, specimen racks (for repository use for reanalysis if necessary) = $400 Note: all sampling events will be represented by three samples since distillations can’t be repeated easily.
Analyses – $125/specimen x 48 specimens = $6,000 (UVA contract bulk specimen rate, indirect costs included)
5 undergraduate students will be assigned to this year long academic credit-earning project. We anticipate finding up to 40 of the most abundant congeners per specimen yielding 1,920 data points that will need some relatively extensive computer time for application of Kraitchman’s equations or least linear squares fitting for accurate determination of molecular structures with precision at the level of a few picometers.
All labor- no charge